CN101818184A - Method for extracting rutin from sophora japonica - Google Patents
Method for extracting rutin from sophora japonica Download PDFInfo
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- CN101818184A CN101818184A CN201010161326A CN201010161326A CN101818184A CN 101818184 A CN101818184 A CN 101818184A CN 201010161326 A CN201010161326 A CN 201010161326A CN 201010161326 A CN201010161326 A CN 201010161326A CN 101818184 A CN101818184 A CN 101818184A
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Abstract
The invention discloses a method for extracting rutin from sophora japonica, which comprises the following steps of: (1) cleaning and drying sophora japonica, putting the sophora japonica into a fermentation tank, adding rutin biotransformation enzymes for closed fermentation for 4-6 hours, and then, transferring the sophora japonica into an extraction tank; (2) adding 4.5 times of mixed solvent of methanol and ethanol into the extraction tank for stirring, extracting and filtering to obtain a filtered solution; (3) distilling the filtered solution, and then, recovering the solvent to obtain rutin extract; and (4) adding 3-5 times of quantity of mixed solvent of acetone, petroleum ether and n-octanol into the obtained rutin extract for conventionally stirring, extracting and filtering, distilling the filtered solution, and recovering the solvent to obtain high-purity rutin finished products. In the invention, the whole extracting process is closed and does not cause environment pollution; the extracting time is short, and the whole extracting and refining operation can be finished only in 16 hours; equipment used for extracting is conventional equipment, thus the enterprise burden can not be increased; and the solvent can be recycled, the production cost is low, the rutin yield is high, and the product purity meets the standard of State Pharmacopoeia and the standard of European Pharmacopoeia 6 (EP6).
Description
Technical field
The present invention relates to a kind of method of from the sophora bud, extracting rutin.
Background technology
Rutin (Rutin) dewaters the synthetic glycosides by the hydroxyl on 3 of the quercetins (Quercetin) and rutinose (Rutinose) (disaccharide of forming for glucose (Glucose) and rhamnosyl (Rhamnose)).Rutin (Rutin) extensively is present in the vegitabilia, has now found that the plant that contains rutin is at least more than 70 kinds, as tobacco leaf, sophora flower, buckwheat and taraxacum etc.Especially the highest with content in Flos Sophorae Immaturus (being the open bud in end of plant Sophora japonica) and the buckwheat, can be used as the raw materials of a large amount of extraction rutins.Rutin is buff powder or superfine needle crystal, contains the termolecular crystal water, and fusing point is 174～178 ℃, 188～190 ℃ of anhydrides.Solubleness: be 1: 10000 in the cold water; In the hot water 1: 200; Cold ethanol 1: 650; Hot ethanol 1: 60; Cold pyridine 1: 12.Be slightly soluble in acetone, ethyl acetate, be insoluble to benzene, ether, chloroform, sherwood oil, be dissolved in alkali and be yellow.Rutin has the effect of vitamin P sample, helps to keep and recover the normal elasticity of capillary vessel, and is main as preventing and treating the auxiliary therapeutical agent of essential hypertension, also can be used for preventing and treating other hemorrhages due to the rutin for want of.
The extracting method of tradition rutin is: sophora bud high temperature was fumigated 30 minutes, be crushed to 40～60 order particles, boiling water is scalded; Pack into then in the diacolation cylinder, about 12 hours, collect percolate with the saturated limewater diacolation, with dilute hydrochloric acid the pH value of percolate is adjusted to 3～4 again, leave standstill, the rutin crystallization is separated out, and obtains rutin runic thing.Because stifling and boiling water is scalded all and can be destroyed rutin with sophora bud high temperature, causes yield to reduce, in the alkali extraction and acid precipitation process, also can destroy the structure of rutin and separate out, and a large amount of sour waters of discharging have brought pollution to environment, deal with very difficulty.Whole leaching process requires processing condition such as high temperature, strong acid and strong base, and the cycle is long, and the three wastes of generation are many, and rutin yield can only reach 18～20%.
Summary of the invention
The object of the present invention is to provide the method for from the sophora bud, extracting rutin that a kind of extracting cycle is short and yield is higher.
For achieving the above object, the present invention can take following technical proposals:
The method of extracting rutin from the sophora bud of the present invention comprises the steps:
The first step: the sophora bud is cleaned oven dry place fermentor tank, add the rutin bio-transformation enzyme of charging capacity 0.1～1%, the back sealed fermenting that stirs changed extractor over to after 4～6 hours;
Second step: in extractor, add the methyl alcohol of 4.5 times of charging capacitys, the solvent that ethanol mixes, stir and extract after 30～40 minutes, filter and obtain filtrate;
The 3rd step: after above-mentioned filtrate distillation, reclaim solvent, obtain the rutin extract;
The 4th step: add the solvent that 3～5 times of amounts are mixed by acetone, sherwood oil and n-Octanol in the rutin extract that obtains in the 3rd goes on foot, ordinary method stirs, extracts, filters, and the filtrate distillation obtains the high-purity rutoside finished product behind the recovery solvent.
Extraction in described second step, filtration number of times at least three times.
Methyl alcohol in described second step in methyl alcohol, the alcohol mixed solvent: ethanol=2: 1.
Acetone in described the 4th step in acetone, sherwood oil and the n-Octanol mixed solvent: sherwood oil: n-Octanol=20: 20: 60.
The invention has the advantages that whole leaching process is airtight, non-environmental-pollution; Extraction time is short, only needs 16 hours can finish whole extractions and refining work; The equipment that uses in the leaching process (fermentor tank, extractor, extractor, thickener, distillation tower, filter etc.) is common equipment, can not increase business burden; Solvent can use repeatedly, and loss is few, and waste residue can be used for feed or fertilizer; Production cost is low, only is 2/3～3/4 of traditional extraction process; Rutin yield is higher than traditional extraction process 40%, and product purity meets state-promulgated pharmacopoeia standard and European EP6 standard.
Embodiment
The method of extracting rutin from the sophora bud of the present invention comprises the steps:
The first step: the sophora bud is cleaned oven dry place fermentor tank, add the rutin bio-transformation enzyme of charging capacity 0.1～1%, the total charge amount in the tank body is less than 70% of tank body capacity, and the back sealed fermenting that stirs changed extractor over to after 4～6 hours;
Second step: the methyl alcohol that in extractor, adds 4.5 times of charging capacitys: the mixed solvent of ethanol=2: 1, stir and extract after 30～40 minutes, filter and obtain filtrate, filter residue extracts three times repeatedly at least;
The 3rd goes on foot: the merging of above-mentioned multiple extraction filtrate is placed in the distillation tower distills, reclaim solvent, obtain the rutin extract;
The 4th step: the rutin extract that obtains in the 3rd step is placed extractor, add 5 times of amounts of rutin extract by acetone: sherwood oil: the mixed solvent of n-Octanol=form at 20: 20: 60, stir according to a conventional method, extract, filter, the filtrate distillation, obtain content 99.9%～101% after reclaiming solvent, moisture 7.5～9.0%, total impurities is less than 3.0% rutin finished product, and the rutin total recovery can reach 30～35%.
Claims (4)
1. a method of extracting rutin from the sophora bud is characterized in that: comprise the steps:
The first step: the sophora bud is cleaned oven dry place fermentor tank, add the rutin bio-transformation enzyme of charging capacity 0.1～1%, the back sealed fermenting that stirs changed extractor over to after 4～6 hours;
Second step: in extractor, add the methyl alcohol of 4.5 times of charging capacitys, the solvent that ethanol mixes, stir and extract after 30～40 minutes, filter and obtain filtrate;
The 3rd step: after above-mentioned filtrate distillation, reclaim solvent, obtain the rutin extract;
The 4th step: add the solvent that 3～5 times of amounts are mixed by acetone, sherwood oil and n-Octanol in the rutin extract that obtains in the 3rd goes on foot, ordinary method stirs, extracts, filters, and the filtrate distillation obtains the high-purity rutoside finished product behind the recovery solvent.
2. the method for extracting rutin from the sophora bud according to claim 1 is characterized in that: the extraction in described second step, filtration number of times at least three times.
3. the method for extracting rutin from the sophora bud according to claim 1 and 2 is characterized in that: the methyl alcohol in described second step in methyl alcohol, the alcohol mixed solvent: ethanol=2: 1.
4. the method for extracting rutin from the sophora bud according to claim 1 and 2 is characterized in that: the acetone in described the 4th step in acetone, sherwood oil and the n-Octanol mixed solvent: sherwood oil: n-Octanol=20: 20: 60.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010161326A CN101818184A (en) | 2010-05-04 | 2010-05-04 | Method for extracting rutin from sophora japonica |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010161326A CN101818184A (en) | 2010-05-04 | 2010-05-04 | Method for extracting rutin from sophora japonica |
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| CN101818184A true CN101818184A (en) | 2010-09-01 |
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| CN201010161326A Pending CN101818184A (en) | 2010-05-04 | 2010-05-04 | Method for extracting rutin from sophora japonica |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500130A (en) * | 2011-10-28 | 2012-06-20 | 四川省砚山中药饮片有限公司 | First-stage rutin extraction equipment |
| CN102807596A (en) * | 2012-08-23 | 2012-12-05 | 四川省砚山中药饮片有限公司 | Method for extracting rutin |
| CN106749454A (en) * | 2015-11-25 | 2017-05-31 | 衡阳市骏杰化工有限公司 | A kind of extracting method of rutin |
| CN107434816A (en) * | 2016-05-25 | 2017-12-05 | 辽宁药联制药有限公司 | One kind extracts rutin method from Ilex Latifolia Thunb |
| CN113115798A (en) * | 2021-04-23 | 2021-07-16 | 北京农学院 | Application of Chinese scholartree in biological control, biological control medicament and preparation method thereof |
| CN114246208A (en) * | 2021-12-29 | 2022-03-29 | 烟台百事特丽特种肥料有限公司 | Method for preparing fruit and vegetable preservative by fermenting and extracting sophora flower buds |
-
2010
- 2010-05-04 CN CN201010161326A patent/CN101818184A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500130A (en) * | 2011-10-28 | 2012-06-20 | 四川省砚山中药饮片有限公司 | First-stage rutin extraction equipment |
| CN102807596A (en) * | 2012-08-23 | 2012-12-05 | 四川省砚山中药饮片有限公司 | Method for extracting rutin |
| CN106749454A (en) * | 2015-11-25 | 2017-05-31 | 衡阳市骏杰化工有限公司 | A kind of extracting method of rutin |
| CN107434816A (en) * | 2016-05-25 | 2017-12-05 | 辽宁药联制药有限公司 | One kind extracts rutin method from Ilex Latifolia Thunb |
| CN113115798A (en) * | 2021-04-23 | 2021-07-16 | 北京农学院 | Application of Chinese scholartree in biological control, biological control medicament and preparation method thereof |
| CN114246208A (en) * | 2021-12-29 | 2022-03-29 | 烟台百事特丽特种肥料有限公司 | Method for preparing fruit and vegetable preservative by fermenting and extracting sophora flower buds |
| CN114246208B (en) * | 2021-12-29 | 2024-04-19 | 烟台固特丽生物科技股份有限公司 | Method for preparing fruit and vegetable preservative through pagodatree flower bud fermentation and extraction |
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Application publication date: 20100901 |